反应详情

DHP (0.67 mL, 7.4 mmol) and CSA (30 mg, 0.12 mmol) were added to a solution of [2-bromo-3-(4-methoxy-benzyloxy)-phenyl]-methanol (2.0 g, 6.1 mmol) in CH2Cl2 (15 mL). The resulting mixture was stirred at rt O/N. 4 Å Molecular sieves (1.0 g) was added and mixture was stirred for 1 h. Sat. NaHCO3 was added and mixture was extracted with CHCl3 (2×50 mL). The organic fractions were washed with H2O (2×25 mL) then brine (50 mL), dried (Na2SO4), and concentrated in vacuo. The residue was purified by flash chromatography (25% EtOAc in hexane) to give the title compound as yellow oil: yield 1.30 g (96%).

1. addition4 Å Molecular sieves (1.0 g) was added
2. stirringmixture was stirred for 1 h
3. extractionmixture was extracted with CHCl3 (2×50 mL)
4. washThe organic fractions were washed with H2O (2×25 mL)
5. dry with materialbrine (50 mL), dried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography (25% EtOAc in hexane)